Process for refining nitrogen trifluoride gas using alkali earth metal exchanged zeolite

a technology of alkali earth metal exchanged zeolite and nitrogen trifluoride, which is applied in the field of process for refining nitrogen trifluoride gas, can solve the problems of inability to refinance, inability to refinance, and inability to refinance, and achieve the effect of high purity nitrogen trifluorid

Active Publication Date: 2010-11-30
HYOSUNG CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0014]The process according to the present invention can effectively produce high purity nitrogen trifluoride, by the removal of CF4.

Problems solved by technology

Active carbon and active alumina, however, is highly disadvantageous in terms of labor and cost because they must be frequently changed with fresh adsorbent or regenerated owing to its poor capacity for adsorbing impurities, which result in an inevitable loss of NF3 gas.
This method, however, is disadvantageous in that an additional desorption process must be conducted, and the water content of the synthetic zeolite must be adjusted to be within a predetermined range.
In addition, the NF3 gas refined by this method has a purity of 93% or less so that it cannot be directly applied to fields requiring high purity.
However, the hydrothermal pretreatment for controlling the porosity of zeolite is difficult to conduct.
In addition, the available time period of the zeolite, that is, the saturation time period, is too short to apply the zeolite method in the commercialized mass purification of nitrogen trifluoride.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0044]Zeolite 3A (commercially available from Aldrich. Inc., particle size 8˜12 meshed, spherical) was slowly added to a 1M solution of a precursor of alkali earth metal in distilled water and well mixed together. The suspension was allowed to react for 6 hours at 80° C. with slow stiffing, followed by recovery of the zeolite 3A through filtration. Thereafter, the zeolite 3A was dried at 130° C. for 6 hours in an oven and then baked at 500° C. for 12 hours to give a zeolite 3A ion-exchanged with an alkali earth metal in an amount of 50 weight %. An X-ray fluorescence spectrometer (XRF) was used to measure the content of the alkali earth metal in comparison with the total metal present inside the zeolite. The results are given in Table 1, below.

preparation example 21

[0045]A zeolite 3A ion-exchanged with alkali earth metal was prepared in a manner similar to that of Preparation Example 1, with the exception of a difference in the type and concentration of the alkali earth metal precursor solution, and the temperature and time period of the stirring. The results are given in Table 1, below.

preparation example 3

[0046]The same procedure as Preparation Example 1 was carried out, with the exception that zeolite 4A was used instead of zeolite 3A to produce a zeolite 4A that is ion-exchanged with alkali earth metal. The results are given in Table 2, below.

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Abstract

Disclosed herein are a process for the refinement of nitrogen trifluoride gas and an adsorbent used therein. A nitrogen trifluoride (NF3) gas including carbon tetrafluoride (CF4) as an impurity is permeated into a bed of the zeolite 3 A, 4A or 5 A which is ion exchanged with alkali earth metal and is thermally treated at 150 to 600° C. for 0.5 to 100 hours so as to selectively adsorb nitrogen trifluoride onto the bed, followed by the desorption of the nitrogen trifluoride therefrom.

Description

TECHNICAL FIELD[0001]The present invention relates, in general, to the refinement of nitrogen trifluoride (NF3) gas and, more particularly, to a process for refining nitrogen trifluoride gas through the removal of carbon tetrafluoride (CF4) therefrom.BACKGROUND ART[0002]In the semiconductor industry, nitrogen trifluoride has a variety of applications, including as a fluorine source for plasma etch, a cleaning agent for CVD reactors, and a dry etchant for semiconductors. Besides, nitrogen trifluoride is useful as a rocket fuel. With the development of the semiconductor industry, the nitrogen trifluoride gas has been in great demand. The increasing demand for a gas without any environmental pollution increased the demand for the nitrogen triflurode gas by geometric progression. As a matter of course, nitrogen trifluoride gas for use in these applications is required to be of high purity.[0003]Nitrogen trifluoride can be prepared by various methods, including the direct fluoridation of...

Claims

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Application Information

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Patent Type & Authority Patents(United States)
IPC IPC(8): B01D53/02
CPCB01D53/02B01J20/186C01B21/0837C01B39/026B01D53/0423B01D53/0462B01D2253/108B01D2253/308B01D2257/2066B01D2258/0216B01D2259/4006B01D2259/401Y02C20/30Y10S95/90Y02P20/151
Inventor PARK, YONG-CHULJEONG, WOO-SIKHYUN, KWANG-CHULLEE, JANG-WONKWON, IK-HYEON
Owner HYOSUNG CHEM CORP
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